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Background Statement forSEMI Draft Document 6084
Revision to SEMI C93-0216 (Preliminary)
GUIDE FOR DETERMINING THE QUALITY OF ION EXCHANGE RESIN USED IN POLISH APPLICATIONS OF ULTRAPURE WATER SYSTEM
Notice: This background statement is not part of the balloted item. It is provided solely to assist the recipient in reaching an informed decision based on the rationale of the activity that preceded the creation of this document.
Notice: Recipients of this document are invited to submit, with their comments, notification of any relevant patented technology or copyrighted items of which they are aware and to provide supporting documentation. In this context, “patented technology” is defined as technology for which a patent has issued or has been applied for. In the latter case, only publicly available information on the contents of the patent application is to be provided.
This is a first revision of C93-0216 which was published as a SEMI Preliminary standard in February 2016. This revision removes its Preliminary status.
The Liquid ChemicalsNA TC Chapter reviewed C93-0216 (Preliminary) and recommended to issue arevision ballot, #6084.
Review and Adjudication Information
Task Force Review / Committee AdjudicationGroup: / UPW / Liquid Chemicals TC Chapter
Date: / Monday, November 7, 2016 / Tuesday, November 8, 2016
Time & Time Zone: / 08:00 AM to 11:00 AM PST / 3:00 PM to 6:00 PM PST
Location: / SEMI HQ / SEMI HQ
City, State/Country: / San Jose, CA/USA / San Jose, CA/USA
Leader(s)/Authors: / Slava Libman (Air-Liquide) / Frank Flowers (PeroxyChem)
Standards Staff: / Inna Skvortsova () / Inna Skvortsova ()
Meeting details are subject to change, and additional review sessions may be scheduled if necessary. Contact Standards staff for more information.
Telephone and web information will be distributed to interested parties as the meeting date approaches. If you will not be able to attend these meetings in person but would like to participate by telephone/web, please contact Standards staff.
Check on calendar of event for the latest meeting schedule.
SEMI Draft Document 6084
Revision to SEMI C93-0216 (Preliminary)
GUIDE FOR DETERMINING THE QUALITY OF ION EXCHANGE RESIN USED IN POLISH APPLICATIONS OF ULTRAPURE WATER SYSTEM
This Standard was technically approved by the Liquid ChemicalsGlobal Technical Committee. This edition was approved for publication by the global Audits and Reviews Subcommittee on February 1, 2016. Available at and in February 2016.
1 Purpose
1.1 This Document describes a Guide for analysis of virgin high-purity ion exchange (HPIX) resin suitable for use in ultrapure water (UPW) polish applications. Further information regarding UPW systems can be found in SEMI F61.
1.2 The Guide focuses on analysis of HPIX resin used in UPW. This Document recommends parameters and test conditions that will minimize the effect of contamination from the resin on the manufacturing process.
1.3 The purpose of the Guide is to avoid prolonged rinse-up of the new HPIX when it is loaded into ion exchange (polish) tanks. The Guide results should be representative of full-scale applications.
2 Scope
2.1 This Document includes recommendations for virgin HPIX resin sample handling and test conditions.
2.2 The Document provides an example of the performance of state-of-the-art resins; the data was obtained following this Guide. However the quality criteria are expected to be determined by the end user based on the user-specific needs.
2.3 It is the intent of this Guide to focus on virgin HPIX resin. The quality parameters assessed, as recommended by this Guide, include quantitative measures of particle contribution, metallic contribution, organics contribution, residue after evaporation (RAE) (nonvolatile residue [NVR]), and broken beads content.
2.4 The Guide takes the wetted-stream performance of virgin HPIX resin into consideration and reflects the current manufacturing processes of the resin manufacturers.
2.5 Leach-out procedures referenced within this Document provide values for both static and dynamic conditions. Although the static leach-out testing is sufficient to determine resin quality, the end user should decide whether to use a dynamic leach-out testing; dynamic testing provides conditions closer to mimicking the actual mixed-bed operation. Choosing either a dynamic leach test or a static leach test is determined by the end user needs. Dynamic leach tests should be used to estimate the rinse-up flush volume. Static leach tests should be used for quality assurance when baseline virgin resin quality has already been established (otherwise use the dynamic leach test to estimate the rinse-up time).
2.6 Only mixed virgin HPIX resin is used for the testing within this Document. When the resin is supplied in nonmixed form (i.e., anionic and cationic), a mixed sample is used for analysis.
2.7 The Guide assumes that the virgin HPIX resin tested is representative of the virgin HPIX resin to be loaded in the mixed-beds tanks. The resin shelf life, storage, and delivery conditions should be taken into account when planning the testing.
2.8 This Guide applies to virgin HPIX resin as well as point of use (POU) HPIX modules intended for use in semiconductor manufacturing equipment and their ancillary equipment.
2.9 This Guide includes recommended analytical testing that the end user can perform; the end user should determine which analyses are required and whether to conduct optional testing.
NOTICE:SEMI Standards and Safety Guidelines do not purport to address all safety issues associated with their use. It is the responsibility of the users of the Documents to establish appropriate safety and health practices, and determine the applicability of regulatory or other limitations prior to use.
3 Limitations
3.1 This Guide applies solely to virgin HPIX resin testing. Quality and performance of the associated equipment (i.e., HPIX beds, piping, piping components) are not included in the Guide.
3.2 Virgin HPIX resin tested by following this Guide is intended for use in the polishing system of (UPW) systems only (i.e., located downstream the UPW tank). These testing conditions may exceed the needs of resin used in primary mixed beds and other less critical applications.
3.3 The Guide is designed to assess contamination from the resin in an ‘as-received’ state; onsite resin handling may add contaminants. The effects of the onsite handling are beyond the scope of this Document, but should be considered by the supplier or user.
3.4 Performance of premixed resin vs. mixed in the lab is expected to be different. The sample should be prepared (i.e., mixed) in the same way it is done for the actual application (premixed by manufacturer vs. mixed onsite).
3.5 This Guide is not intended to supersede customer specifications.
3.6 Virgin HPIX resin samples tested under the conditions recommended by this Guide may vary in their performance from the resin used in the actual UPW system. Resin inconsistency should be addressed with the resin supplier or by conducting a statistical analysis of the resin quality data.
3.7 The accuracy of the data generated by this Guide is limited to the accuracy of the analytical techniques used to measure resin quality.
3.8 Tolerances in the figures used in the Guide (such as flow rate, concentration, etc.) are ±10% unless otherwise stated.
3.9 This Guide application is limited to the ambient temperature UPW system. Other applications, such as hot UPW systems or different treatment solvent have not been considered in this Document.
3.10 The reference data provided in Appendix 2 is representative for 2014 state-of-the-art resin quality and may not be fully representative for future state-of-the-art resin.
3.11 Limited experience and data are currently available in application of this Guide. Additional reproducibility studies may need to be conducted by the end user when defining performance criteria for the resin tested.
3.12 This Guide recommends a simplified option of the static leach test vs. dynamic leach test, mimicking actual polish mixed operation. Although data in Appendix 2 suggested that static leach test may be representative for the analysis of the resin performance under dynamic conditions, the choice of the testing should take into account the fact of the limited amount of data collected by the date of publication of this Document.
4 Referenced Documents
4.1 SEMI Standards and SafetyGuidelines
SEMI E49 —Guide for High Purity and Ultrahigh Purity Piping Performance, Subassemblies, and Final Assemblies
SEMI F40 — Practice For Preparing Liquid Chemical Distribution Components for Chemical Testing
SEMI F57 — Specification for Polymer Materials and Components Used in Ultrapure Water and Liquid Chemical Distribution Systems
SEMI F61 — Guide for Ultrapure Water Systems used in Semiconductor Processing
SEMI F63 —Guide for Ultrapure Water Used in Semiconductor Processing
SEMI F104 —Particle Test Method Guide for Evaluation of Components Used in Ultrapure Water and Liquid Chemical Distribution Systems
SEMI S2 — Environment, Health, and Safety Guideline for Semiconductor Manufacturing Equipment
4.2 ASTMStandards[1]
ASTM D4779 — Standard Test Method for Total, Organic, and Inorganic Carbon in High Purity Water by Ultraviolet (UV) or Persulfate Oxidation, or Both, and Infrared Detection (Withdrawn 2002)
ASTM D5544 — Standard Test Method for On-line Measurement of Residue After Evaporation of High-Purity Water
ASTM D5904 — Standard Test Method of Total Carbon, Inorganic Carbon, and Organic Carbon in Water by Ultraviolet, Persulfate Oxidation and Membrane Conductivity Detection
4.3 ISOStandard[2]
4.4 ISO 14644-1 — Cleanrooms and Associated Controlled Environments – Part 1: Classification of Air Cleanliness by Particle Concentration
4.5 FederalStandard[3]
FED STD 209E — Airborne Particulate Cleanliness Classes in Cleanrooms and Clean Zones
4.6 OtherDocuments
International Technology Roadmap for Semiconductors (ITRS)[4]
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
5 Units
5.1 Parts per million (ppm) is equivalent to µg/mL or mg/L, where 1 L approximately equals 1 kg.
5.2 Parts per billion (ppb) is equivalent to ng/mL or µg/L, where 1 L approximately equals 1 kg.
5.3 Parts per trillion (ppt) is equivalent to pg/mL or ng/L, where 1 L approximately equals 1 kg.
5.4 Micrometer is a unit of length equal to one millionth of a meter, or one thousandth of a millimeter.
6 Terminology
NOTE 1:General terms for UPW systems can be found in SEMI F61.
6.1 General terms and acronyms used in this Standard are listed below and may be defined in SEMI F61.
6.2 Abbreviations and Acronyms
6.2.1 DMA — differential mobility analyzer
6.2.2 HPIX— high-purity ion exchange
6.2.3 HPW— high purity water
6.2.4 ICP-MS — inductively coupled plasma mass spectrometry
6.2.5 ITRS — International Technology Roadmap For Semiconductors
6.2.6 LC-OCD— liquid chromatography with organic carbon detector
6.2.7 LNS— Liquid Nano-particle Sizing System; an example of a particle size distribution analyzer (PSDA) used for the validation testing, see results in Appendix 2.
6.2.8 LPC— laser particle counter
6.2.9 NRM — nonvolatile residue monitor
6.2.10 NVR — nonvolatile residue
6.2.10.1 Discussion — NVR is also called residue after evaporation (RAE).
6.2.11 PFA— perfluoroalkoxy
6.2.12 POU — point of use
6.2.13 PSDA — particle size distribution analyzer
6.2.14 PVDF— polyvinylidene fluoride
6.2.15 RAE— residue after evaporation
6.2.15.1 Discussion — RAE is also called nonvolatile residue (NVR).
6.2.16 SEM— scanning electron microscope
6.2.17 TOC — total organic carbon
6.2.18 UPW — ultrapure water
6.3 Definitions
6.3.1 background — the contaminant concentrations in the test system reported by analyzers, such as a particle size distribution analyzer (PSDA), nonvolatile residue monitor (NRM), total organic carbon (TOC), and others. Background includes contaminant contributions from the ultrapure water (UPW) and the test equipment components.
6.3.2 delta measurement— the ultrapure water (UPW) contaminant concentration difference between the inlet of the resin column and the outlet of the resin column.
6.3.3 dynamic leach test skid— the system providing resin-evaluation test analysis. The test skid includes piping, resin column, flow meters, pressure gauges, valves, regulators, sample ports, etc. Figure 1 provides illustration of the skid.
6.3.4 virgin HPIX resin — an unused, high purity ion exchange (HPIX) resin that has not been regenerated.
7 Dynamic Leach Test Skid Configuration
7.1 The dynamic leach test skid should be made of high-purity components, meeting SEMI F57 quality requirements. Figure 1 presents the recommended configuration of the skid. The ion exchange column is made of polyvinylidene fluoride (PVDF)with perfluoroalkoxy (PFA)tubing connecting the column to the UPW system and analytical equipment.
Figure 1
General Test Schematic Diagram for Dynamic Leach Test
7.2 Minimum operating pressure should be sufficient to feed the instruments downstream of the ion exchange column, typically 25 psig(172 kPa). The pressure gauges and flow meters should be installed downstream or side stream to avoid contamination. Pressure on the feed side to the column should be 207 to 310 kPa (30to45 psig) to reduce potential micro bubble formation. The high-pressure limit depends upon the materials of construction (for safety and leak prevention).
7.3 Ultrapure, low-particle, low-TOC, low-shedding piping systems should be used in all wetted flow paths from the UPW source to the dynamic leach test skid to ensure that adequate water qualityis maintained. Consider the recommendations within SEMI E49when designing and assembling the system.
7.4 Protect the test system from excessive vibration, which could lead to high particle-background counts.
7.5 Minimum operating pressure downstream of the dynamic leach test skid should be 138 kPa (20 psig) during testing to avoid gas bubbles.
7.6 The UPW should be in compliance with the following minimum guidelines:
7.6.1 Temperature — 23 ± 5°C (77 ± 9°F).
7.6.2 Resistivity — ≥18 MΩ·cm at 25°C (77°F).
7.6.3 TOC —2 ppb.
7.6.4 NVR — <0.2 ppb.
7.6.5 Maximum Recommended Particle-Concentration Background Level — <1 particle/mL (≥0.05µm). Background particle levels measured by PSDA are dictated by the resin performance expectations (see Figure A2-2, Appendix 2).
7.6.6 To ensure a stable background level, before beginning the test install and rinse the ion exchange column inan enclosed ISO Class 7 (per current revision of ISO 14644-1, roughly equivalent to FED STD 209E Class 10,000), or better, environment. Follow procedures necessary to maintain ISO Class 7, or better, when handling any part of the test system, or during the testing. End users requiring more exacting testing should consider following more stringent testing requirements.
7.6.7 Instrumentation, including flow meters, pressure gauges/transducers and temperature sensors, should be calibrated in accordance with the manufacturers’ procedures and frequency.
7.6.8 Bubbles cause metrology errors; orient the test column and the plumbing between the components under test to limit bubble entrapment. Position the ion exchange column vertically and vent the test skid to prevent gas accumulation and bubble formation. Provisions should be included in the test stand to capture and divert bubbles before they enter the instrumentation supply lines.
NOTE 2:UPW flow through the ion exchange column should be from the top to the bottom to prevent resin separation.
8 Sample Recommendations
8.1 Test a representative ion exchange virgin resin sample from the batch under consideration.
8.2 To take a virgin resin sample from the drums at the end user location, it is recommended to follow this procedure:
8.2.1 Avoid construction and other maintenance activities in the area where the sample is taken.
8.2.2 Rinse the outside of the drums with high purity water (HPW) before opening to remove contamination collected during transport and storage. Allow the water to drip off the drums.
8.2.3 Don clean room suit and low-zinc gloves.
8.2.4 Prepare clean bags for the resin sampling and shipping. Use double-bagged packaging (the inner bags should be qualified for low background level of particles, while the outer bags should have low gas permeability).
8.2.5 Take resin from a previously unopened drum.
8.2.6 Open a representative drum and open the protective bags inside the drum.
8.2.6.1 If resin prepared for testing is supplied from different batches or was stored under different conditions, you may need to test more than one sample.
8.2.6.2 If the amount of resin in a single drum is <10% of the total amount of the resin to be used, you may need to sample more than one drum in order to obtain representative results.
8.2.7 Sample resin immediately after you open the drum.
8.2.7.1 Take the sample from the top of the drum to prevent excess liquid from being taken with the sample.
8.2.7.2 Remove approximately 5 cm (2 in.) of the upper resin layer.
8.2.7.3 Take 1 L of the resin sample for a static leach test and 1 L for a dynamic leach test.
8.2.7.4 Minimize exposure of the resin sample to ambient contamination.
8.2.7.5 Use gentle motion to avoid damaging the resin beads.
8.3 Place the resin in a prepared clean bag and seal the bag.
8.4 Wrap the resin sample in bubble wrap to protect it during shipping.
8.5 Place the resin sample in a cooler and ship to the lab using fast, direct delivery (do not exceed one week in shipment). Add ‘FRAGILE’ sticker.
NOTE 3:Resin sample handling and packaging may impact the test results. Samples submitted for testing should reflect standard practices of handling and packaging by the resin manufacturer in accordance with the typical manufacturing processes.
9 Test Methodology
9.1 Leach-OutParameters
9.1.1 This Document does not provide specific quality requirements for leachable parameters. The end user should define quality requirements based upon the process-specific sensitivity to contamination, the ion exchange polish system design, and the data provided in Appendix 2. The results in Appendix 2 are based on the benchmarking study and indicate the actual range of performance of typical resins used in ion exchange polish applications.
9.1.2 Success criteria considerations for TOC and particle release. Contamination by organic compounds causes silicon oxidation. It also affects etching uniformity, wafer and mask cleaning, adhesion of the resist, gate oxide breakdown voltage, epitaxial growth, atomic layer deposition (ALD), and chemical vapor deposition (CVD) of silicon nitride or other thin film deposition.